U.S. patent number 5,433,890 [Application Number 08/277,125] was granted by the patent office on 1995-07-18 for rubber and polymer preservative and protectant.
This patent grant is currently assigned to First Brands Corporation. Invention is credited to Kenneth L. Meyer, Edward T. Turner, Richard L. Wolstoncroft.
United States Patent |
5,433,890 |
Meyer , et al. |
July 18, 1995 |
Rubber and polymer preservative and protectant
Abstract
An aqueous polymer preservative and protectant composition
containing a silicone emulsion, an aminofunctional silicone
emulsion, a film forming thickening agent and a polyol.
Inventors: |
Meyer; Kenneth L. (Yorktown
Heights, NY), Turner; Edward T. (Danbury, CT),
Wolstoncroft; Richard L. (Mount Kisco, NY) |
Assignee: |
First Brands Corporation
(Danbury, CT)
|
Family
ID: |
24386659 |
Appl.
No.: |
08/277,125 |
Filed: |
July 19, 1994 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
|
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596269 |
Oct 12, 1990 |
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Current U.S.
Class: |
427/355; 106/10;
106/287.11; 106/287.13; 106/287.16; 106/3; 106/9; 252/380;
516/55 |
Current CPC
Class: |
C09G
1/04 (20130101); C09G 1/16 (20130101) |
Current International
Class: |
C09G
1/00 (20060101); C09G 1/16 (20060101); C09G
1/04 (20060101); C09G 001/10 (); C09G 001/12 () |
Field of
Search: |
;252/309,380,38
;106/3,6,287.11,287.13,287.16,10 ;427/355,369 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Geist; Gary L.
Assistant Examiner: Fee; Valerie
Attorney, Agent or Firm: Wamer; Gary L.
Parent Case Text
This application is a Continuation of prior U.S. application Ser.
No. 07/596,269 filed Oct. 12, 1990, abandoned.
Claims
What is claimed:
1. A composition for treating a surface comprising:
(i) between about 20 and about 40 weight percent water;
(ii) between about 50 and about 60 weight percent silicone emulsion
containing about 20 to about 40 weight percent
dialkylpolysiloxane;
(iii) between about 0.5 and about 5 weight percent aminofunctional
silicone emulsion containing 20 to 40 weight percent
aminofunctional polysiloxane;
(iv) between about 2 and about 8 weight percent of a polyol;
(v) between about 1 and about 5 weight percent acrylic copolymer
emulsion containing between about 20 and about 40 weight percent
acrylic copolymer and between about 0.1 and about 1 weight percent
morpholine;
(vi) between about 0.01 and about 1 weight percent of a
bactericide; and
wherein said weight percents are based upon the total weight of the
composition.
2. A composition according to claim 1 wherein said surface is
selected from the group consisting of rubber and polymeric
materials.
3. A composition according to claim 2 or claim 1 wherein said
rubber is selected from the group consisting of natural rubber and
synthetic rubber.
4. A composition according to claim 2 or claim 3 wherein said
polymeric materials are vinyl polymeric materials.
5. A composition for treating a rubber or a vinyl polymer surface
wherein said composition comprises:
(i) between about 30 and about 35 weight percent water;
(ii) between about 55 and about 60 weight percent silicone emulsion
containing about 35 weight percent dialkylpolysiloxane;
(iii) between about 1.0 and 2.0 weight percent aminofunctional
silicone emulsion containing about 35 weight percent
aminodimethylpolysiloxane;
(iv) between about 3 and about 7 weight percent propylene
glycol;
(v) between about 2 and about 4 weight percent acrylic copolymer
emulsion containing between about 25 and about 35 ,weight percent
acrylic copolymer and between about 0.3 and about 0.5 weight
percent morpholine; and
(vi) between about 0.1 and about 0.3 of a mixture of 16 weight
percent water, 19 weight percent 1,2 benziosothiazolin 3-one and 65
weight percent dipropylene glycol; and
wherein said weight percents are based upon the total weight of the
composition.
6. A composition according to claim 1 or claim 5 wherein said pH of
said composition is between about 6.5 and about 9.0.
7. A composition according to claim 6 wherein said pH of said
composition is between about 7.5 and about 8.5.
8. A composition according to claim 1 wherein an antibactericide
agent to inhibit the attack of bacteria is present in an effective
amount.
9. A composition according to 1 wherein said silicone fluid is a
dimethylpolysiloxane and said aminofunctional silicone fluid is an
aminofunctional dimethylpolysiloxane.
10. A process for treating a surface comprising:
(i) wetting said surface with a composition selected from the group
of compositions as set forth in claim 1;
(ii) allowing said composition to penetrate said surface for an
effective period of time:
(iii) lightly wiping said surface after said effective period of
time.
11. A process according to claim 10 wherein said steps (i), (ii)
and (iii) are carried out a second time.
12. A process according to claim 11 wherein said steps (i), (ii)
and (iii) are carried out a third time.
13. A process according to claim 10 wherein said composition is as
set forth in claim 2.
14. A process according to claim 10 wherein said composition is as
set forth in claim 2.
15. A process according to claim 10 wherein said composition has a
viscosity between about 8000 centipoise and about 12,000
centipoise.
16. A process according to claim 15 wherein said pH of said
composition is between about 6.5 and about 9.0.
17. A process according to claim 10 wherein said effective period
of time is up to 24 hours.
18. A process according to claim 17 wherein said effective period
of time is less than 2 hours.
19. A composition according to claim 5 wherein said surface is
selected from the group consisting of rubber and polymeric
materials.
20. A process according to claim 10 wherein said composition is as
set forth in claim 3.
21. A composition for treating rubber and polymeric material
consisting essentially of:
(i) between about 20 and about 40 weight percent water;
(ii) between about 50 and about 60 weight percent silicone emulsion
containing about 20 to about 40 weight percent
dimethylpolysiloxane;
(iii) between about 0.5 and about 5 weight percent aminofunctional
silicone emulsion containing 20 to 40 weight percent
aminofunctional polysiloxane;
(iv) between about 2 and about 8 weight percent of a polyol,
preferably propylene glycol;
(v) between about 1 and about 5 weight percent acrylic copolymer
emulsion containing between about 20 and about 40 weight percent
acrylic copolymer and between about 0.1 and about 1 weight percent
morpholine;
(vi) between about 0.01 and about 1 weight percent of a mixture of
water, 1, 2 benziosothiazolin 3-one and dipropylene glycol wherein
the weight ratio of 1, 2 benziosothiazolin 3-one to dipropylene
glycol is between about 1:10 and about 10:1; and
wherein said weight percents are based upon the total weight of the
composition.
Description
FIELD OF THE INVENTION
The instant invention relates to an improved composition and method
for the treatment of rubber, polymer and other surfaces.
BACKGROUND OF THE INVENTION
The use of protective surface compositions is well known in the
prior art and is commercially demonstrated by the availability of
various products sold under the trademarks SON-OF-A-GU.RTM. (a
trademark of First Brands Properties Inc.) and ARMOR ALL.RTM. (a
trademark of Armor All Products Corporation). The aforementioned
products are well known as providing a silicone-oil based spray-on
protectant to provide gloss (an asthetic appearance property) and a
protectant film to rubber polymer, and other surfaces.
Representative of the well known use of such protectant products is
for use on automotive parts such as automobile tires, vinyl tops,
vinyl dashboards, vinyl upholstery, rubber sealing strips, rubber
and or polymer bumpers and the like and, also, their use on
synthetic rubbers, wood, painted surfaces, leather and the like in
the home.
The nature of such protectant compositions is generally known from
the prior art. For example, the packaging for ARMOR ALL.RTM. brand
protectant lists U.S. Pat. Nos. 3,956,174 and 4,133,921 as covering
the commercial product. U.S. Pat. No. 3,956,174 discloses a
preservative composition consisting essentially of an emulsion of
at least one water emulsifiable organopolysiloxane fluid having a
viscosity of from about 100 to about 10,000 centistokes and, based
on the weight of the polysiloxane fluid from about 65% to about
5,000% by weight of water: and from about 15% to about 65% by
weight based on the weight of the polysiloxane fluid of at least
one water miscible polyol compound. In addition, incorporation of
diethylene glycol (as a polyol) and glycerin (as a polyol) are
stated to be beneficial. In fact, claims 1, 2, 4 and 5 of U.S. Pat.
No. 3,956,174 were disclaimed by the patentee whereby only a
composition containing the aforementioned organopolysiloxane,
diethylene glycol and glycerin is covered by U.S. Pat. No.
3,956,174. U.S. Pat. No. is a division of U.S. Pat. No. 3,956,174
and discloses the process of applying the
organopolysiloxane/diethylene glycol/glycerin composition of U.S.
Pat. No. 3,956,174 to a surface to preserve and renew the surface.
U.S. Pat. No. 4,347,333 discloses an emulsion coating composition
(emulsion) containing silicone fluids, a cleaning solvent, water,
surfactant and an acrylic polymer which is soluble in the cleaning
solvent. The cleaning solvent is present in an amount from about
5-65% by weight if the emulsion is an oil-in-water emulsion and
from about 15-90% by weight if the emulsion is a water-in-oil
emulsion. At column 3, line 22, to column 4,line 8 these required
solvents are described as having good cleaning characteristics.
Representative solvents are stated to include hydrocarbons and
particularly isoparaffinic hydrocarbons, naphtha, Stoddard solvent,
kerosene, turpentine, aliphatic hydrocarbons and cycloaliphatic
hydrocarbons.
In addition to U.S. Pat. Nos. 3,956,174 and 4,133,921, the patent
prior art discloses other preservative and/or coatings for rubber
or vinyl surfaces. U.S. Pat. No. 3,527,723 discloses a coating
composition containing about 0.55% to about 10 by weight emulsified
organopolysiloxane oil and from 1% to about 20% by weight on an
active resin basis of water reducible polyester resin having a set
time of less than about 8 hours and a cure temperature from about
32 degree F. to about 120 degree F. and, optionally, a drying
agent. Canadian Patent No. 1,176,828 discloses ultraviolet
absorbent silicone based water emulsions for vinyl polishes
comprising a polydimethylsiloxane oil or a blend of oils,
sufficient water to form an aqueous continuous phase of said
emulsion, an emulsifying agent and a silicon oil soluble
ultraviolet light absorbing agent.
Although the preservative and treating compositions of the prior
art have been useful in treating rubber and polymer surfaces, there
is a continuing need for improving both the appearance and
protection imparted by use of these products. The instant invention
relates to a novel rubber and polymer preservative and protectant
which provides long lasting gloss to treated surfaces and provides
for improved abrasion protection over commercially available rubber
and polymer preservatives and protectants.
SUMMARY OF THE INVENTION
The compositions for treating a surface of the instant invention
comprise:
(i) a major amount of water:
(ii) an effective amount of a silicone emulsion containing a
dialkylpolysiloxane emulsified in water:
(iii) an effective amount of an aminofunctional silicone emulsion
containing an aminofunctional silicone emulsified in water:
(iv) an effective amount of a polyol;
(v) an effective amount of a film forming thickening agent;
(vi) optionally, an effective amount of anti-bacterial agent.
In a further embodiment the instant composition for treating a
surface comprises concentrations for components (i) to (vi) are as
follows:
(i) between about 20 and about 40 weight percent water;
(ii) between about 50 and about 60 weight percent silicone emulsion
containing about 20 to about 40 weight percent
dimethylpolysiloxane;
(iii) between about 0.5 and about 5 weight percent aminofunctional
silicone emulsion containing 20 to 40 weight percent
aminofunctional polysiloxane;
(iv) between about 2 and about 8 weight percent pf a polyol,
preferably propylene glycol;
(v) between about 1 and about 5 weight percent acrylic copolymer
emulsions containing between about 20 and about 40 weight percent
acrylic copolymer and between about 0.1 and about 1 weight percent
morpholine; and
(vi) optionally, between about 0.01 and about 1 weight percent of a
mixture of water, 1, 2 benziosothiazolin 3-one and dipropylene
glycol wherein the weight ratio of 1, 2 benziosothiazolin 3-one to
dipropylene glycol is between about 1:10 and about 10:1.
In a further embodiment the instant composition for treating a
surface comprising a rubber or a vinyl polymer and the
concentrations of components (i) to (vi) are as follows:
(i) between about 30 to about 35 weight percent water;
(ii) between about 50 to about 60 weight percent silicone emulsion
containing between about 20 to about 35 weight percent
dimethylpolysiloxane;
(iii) between about 1.0 and 2.0 weight percent aminofunctional
silicone emulsion containing about 35 weight percent
aminofunctional dimethylpolysiloxane.;
(iv) between about 3 and about 7 weight percent propylene
glycol;
(v) between about 2 and about 4 weight percent acrylic copolymer
emulsion containing between about 25 and about 40 weight percent
acrylic copolymer and between about 0.3 and 0.5 morpholine; and
(vi) optionally, between about 0.1 and about 0.3 of a mixture of 16
weight percent water, 19 weight percent 1,2 benziosothiazolin 3-one
and 65 weight percent dipropylene glycol.
The compositions of the instant invention provide improved gloss
and resistance to surface abrasion over commercial protectant
compositions currently available and based upon the use of only
dimethysiloxane fluids as the active protectant ingredient.
DETAILED DESCRIPTION OF THE INVENTION
The instant invention relates to novel preservative and protectant
compositions for rubber and polymer surfaces. Such preservatives
and protectants are widely used by consumers in both automotive and
home applications to both improve the appearance of rubber,
polymer, wood, leather, plexiglass, and similar surfaces and to
provide a protective film for such surfaces.
The instant invention relates to a novel combination of chemical
components which have been observed to provide surprising
improvements in the gloss appearance of rubber and polymer surfaces
and the ability of the treated surface to maintain the gloss.
Further, the instant compositions have been observed to provide
improved resistance to abrasion whereby the treated surface is
protected from mild abrasive forces when effective amounts of the
components are combined.
The instant compositions generally comprise:
(i) a major amount of water;
(ii) an effective amount of a silicone emulsion containing
dimalkylpolysiloxane emulsified in water:
(iii) an effective amount of an aminofunctional silicone emulsion,
preferably containing an aminofunctional dimethylpolysiloxane.;
(iv) an effective amount of a polyol;
(v) an effective amount of a film forming thickening agent,
preferably an acrylic copolymer emulsion containing an acrylic
copolymer and morpholine: and
(vi) optionally, an effective amount of a bactericide, preferably a
mixture of 16 weight percent water, 19 weight percent 1.2
benziosothiazolin 3-one and 65 weight percent dipropylene
glycol.
In a further embodiment the instant compositions for treating a
surface have concentrations of components (i) to (vi) which are as
follows:
(i) between about 20 and about 40 weight percent water:
(ii) between about 50 and about 60 weight percent silicone emulsion
containing about 20 to about 40 weight percent
dimethylpolysiloxane:
(iii) between about 0.5 and about 5 weight percent aminofunctional
silicone emulsion containing 20 to 40 weight percent
aminofunctional polysiloxane;
(iv) between about 2 and about 8 weight percent of a polyol,
preferably propylene glycol;
(v) between about land about 5 weight percent acrylic copolymer
emulsion containing between about 20 and about 40 weight percent
acrylic copolymer and between about 0.1 and about 1 weight percent
morpholine; and
(vi) optionally, a bactericide, preferably between about 0.01 and
about 1 weight percent of a mixture of water, 1, 2
benziosothiazolin3-one and dipropylene glycol wherein the weight
ratio of 1, 2 benziosothiazolin 3-one to dipropylene glycol is
between about 1:10 and about 10:1.
In a further embodiment the instant compositions are especially
beneficial for treating a surface which is rubber or a vinyl
polymer and said concentrations of (i) to (vi) are as follows:
(i) between about 30 to about 35 weight percent water:
(ii) between about 55 and to about 60 weight percent silicone
emulsion having 35 weight percent dimethylpolysiloxane;
(iii) between about 1.0 and about 2.0 weight percent
aminofunctional silicone emulsion having 35 weight percent
aminofunctional dimethylpolysiloxane;
(iv) between about 3 and about 7 weight percent propylene
glycol;
(v) between about 2 and about 4 weight percent acrylic copolymer
emulsion containing between about 25 and about 35 crosslinked
acrylic copolymers and between about 0.3 and about 0.5 weight
percent morpholine; and
(vi) between about 0.3 and about 0.5 weight percent of a mixture of
16 weight percent water, 19 weight percent 1.2 benziosothiazolin
3-one and 65 weight percent dipropylene glycol.
The silicone emulsion is an organopolysiloxane fluid and are
commonly referred to in the art as silicone fluids. They comprise
diaikylpolysiloxane fluids, generally dimethylpolysiloxane fluids
of the general formula: ##STR1## where n is the number of repeating
units. The properties and commercial availability of such
dimethylsilicones is well known in the art as evidenced in Table I
(columns 3 and 4) and at column 4, line 32 to column 5, line 20 of
U.S. Pat. No. 3,956,174 and column 3, line 45 to column 5, line 21
of U.S. Pat. No. 4,133,921, said referenced passages being
incorporated herein by reference. Representative of such useful
dimethylsilicone emulsions is an emulsion available under the trade
designation UCC LE-46 which contains 35 percent by weight
dimethylpolysiloxane emulsified in water. UCC LE-46 is available
from Union Carbide Plastics and Chemicals Corporation, Danbury,
Conn. Typical properties of UCC LE-46 are:
UCC LE-46 Typical Properties: 35 weight-percent
dimethylpolysiloxane; Viscosity of contained oil at 25 degrees C.:
10,000 cSt; Emulsion System: Nonionic.
The aminofunctional silicone fluid is an emulsion of an
aminofunctional silicone fluid emulsion and is preferably an
aminofunctional dimethylpolysiloxane fluid. A description of such
aminofunctional silicone fluid may be found at U.S. Pat. No.
3,801,572: U.S. Pat. No. 4,246,029, at column 2, line 41 to column
8, line 49; U.S. Pat. No. 4,247,330, at column 2, line 44 to column
7, line 24; U.S. Pat. No. 4,509,981 at column 3, line 24 to column
6, line 48; and U.S. Pat. No. 4,618,689:, such aforementioned
passages of said patents incorporated by reference. A particularly
useful aminofunctional silicone fluid emulsion is available from
General Electric Corporation under the trade designation GE SM-2059
and contains 35 percent by weight aminofunctional
dimethylpolysiloxane emulsified in water.
It has been observed that the combination of the silicone fluid
emulsion (e.g., UCC LE-46) and the aminofunctional silicone fluid
(e.g. GE SM-2059) provide benefits as to cost of manufacture,
appearance enhancement (commonly referred to as "gloss") and
abrasion protection not provided by preservative and protectant
compositions containing only silicone fluid(s). The benefits of the
instant combination of silicone fluid emulsion and aminofunctional
silicone fluid emulsion derive from their ability to interact at
the surface being treated to provide dual moleties for interaction
with the treated surface and to act upon the surface for an
extended period at the surface owing to high viscosity of the
composition. The instant compositions provide numerous benefits to
the surfaces they are employed to treat, including softening of
vinyl and rubber surfaces, surface lubricity, surface gloss and
resistance to wetting by water.
The aforementioned concentrations of silicone fluid and
aminofunctional silicone fluid are given as weight percents of
emulsions having a range of active silicone fluid or
aminofunctional silicone fluid. It will be understood by those
skilled in the art that the concentration of active silicone fluid
or aminofunctional silicone fluid may be provided by employing
emulsions having different amounts of silicone fluid or
aminofunctional silicone fluid and such are included herein.
The instant composition additionally contains an effective amount
of one or more polyols. The preferred polyol is 1,2- or 1,3-
propylene glycols and mixtures thereof. Other representative
polyols include: diethylene glycol: 1,4 - butylene glycol:
2,3-butylene glycol: 1,3 - butylene glycol: 1,2,6 - hexanetriol:
dipropylene glycol: tetramethylene glycol: pentaerythritol:
dipentene glycol: tetraethylene glycol: dimethyhexanediol: 2,2 -
dimethyl - 1,3 - butanediol: dimethyloldioxane: tetraethylene
glycol: ethylene glycol: liquid polyethylene glycols, and liquid
polypropylene glycols.
The instant compositions also contains effective amounts of a film
forming thickening agent such as an acrylic copolymer emulsion
available from Rohm and Haas Company under the trade designation
ACRYSOL ABE-60. Morpholine (tetrahydro 1,4 oxazine) is preferably
added to the ACRYSOL ASE-60 and acts as a pH activating agent for
the acrylic polymer and acts to form a water resistant film surface
as the morpholine evaporates from the treated surface. Further, the
film forming thickening agent provides an additional increase in
the viscosity of the instant compositions to provide compositions
having an effective viscosity between about 6000 and about 15,000
centistokes and preferably about 8,000 centistokes and about 12,000
centistokes. Compositions having a viscosity in the aforementioned
range are typically referred to as lotions owing to their thickness
and inability to be applied as a spray. The combination of ACRYSOL
ASE-60 as the film forming thickening agent with morpholine as a pH
activating agent for ACRYSOL ASE-60 has been observed to provide a
novel film forming combination when employed in the instant
compositions whereby the silicone fluid and aminofunctional
silicone fluid have improved retention on the treated surface.
Although the ACRYSOL ASE-60 emulsion is initially hydroscopic in
nature, upon being combined with morpholine the resulting dried
combination has an improved resistance to water over ACRYSOL ABE-60
alone, when both are compared as components of the instant
compositions. ACRYSOL ABE-60 is generally characterized as
containing 29 (.+-.0.5) weight percent crosslinked acrylic
copolymer, a pH of 3.5, viscosity as 5 percent sodium salt of
25,000 cps and having a anionic colloidal charge.
The instant compositions beneficially contain an antibacterial
agent to inhibit the attack of bacteria on the emulsifiers in the
silicone fluid and aminofunctional silicone fluid. A particularly
useful antibacterial agent is sold under the trade designation
PROXEL GXL and comprises 19 percent by weight 1,2 benziosothiazolin
3-one, 65 percent by weight dipropylene glycol and 16 percent by
weight water. Other known antibacterial agents (often referred to
as "preservatives" or "biocides") may be employed, including GIVARD
(dimethoxane).
In addition to the aforementioned components, the instant
compositions may optionally contain effective amounts of known
additives, including but not limited to: corrosion inhibitors;
dyes; fragrances, ultraviolet light absorbers; antifoaming agents:
antistatic agents; thickening agents (e.g., xanthan gum, cellulose,
methylcellulose, pectin and the like). These optional components
may be effectively added to modify the appearance, smell or provide
an additional property to the composition by addition of an
optional additive possessing a known performance property.
The pH of the instant compositions are typically between about 6.5
and about 9 and preferably are between about 7.5 and 8.5.
The process by which the instant compositions are employed are well
known in the art. Simply stated the process involves applying,
e.g., by wiping or otherwise physically applying the composition to
a surface (preferably a previously cleaned surface), allowing the
composition to be maintained in contact with the surface for an
effective period of time for the composition to penetrate the
surface. An effective time is typically less than two (2) hours
with an effective treatment period between about 0.15 hours and
about one (1) hour being typical. Although the benefits of the
instant invention may be obtained with effective treatment times of
less than two (2) hours, further benefits may often be obtained by
employing longer treatment periods up to 24 hours. After the
effective treatment period the treated surface is lightly rubbed
with a soft cloth to remove excess composition. The treatment
process may then be repeated, since it has been observed that
additional treatments with the composition will result in the
adherence of additional composition to the treated surface.
Surfaces treated with compositions according to this invention have
a glossy appearance and have resistant to abrasion. Surfaces
appropriate for treatment with the compositions of this invention
include, but are not limited to, natural rubbers, synthetic rubbers
and polymer materials such as vinyl polymers (such as vinylchloride
polymers), polyester, polypropylene, woods, leathers, painted
surfaces, plexiglass and the like.
EXAMPLES
The following examples are set forth to further exemplify the
invention and are not intended to be limiting thereof:
Preparation of Instant Compositions for Examples 1,. 2, 3 and 4
A composition according to the instant invention was prepared for
use in the examples, having the following composition:
______________________________________ COMPOSITION A* Component
Weight Percent ______________________________________ Water 32.89
Silicone Emulsion (UCC LE-46) 57.00 Aminofunctional Silicone 1.50
Emulsion (GE SM2059) Acrysol ASE 60 3.00 Propylene Glycol 5.00
Morpholine 0.45 Proxel GXL** 0.16
______________________________________ *Viscosity approximately
9000 centistokes with a pH of about 8. ** Added with UCC LE46
silicone fluid emulsion.
Composition A is prepared by placing the ingredients in a
thoroughly sanitized stainless steel tank by:
1. adding the water to the tank and commencing moderate
stirring:
2. adding the Proxel GXL:
3. adding the silicone emulsion (UCC LE-46) and stirring for 20
minutes;
4. adding the propylene glycol:
5. adding the aminofunctional silicone fluid (GE SM2059):
6. adding the ACRYSOL ASE-60;
7. adding the morpholine; and then
8. increasing the stirring rate of product as it thickens to
maintain movement at the edges of the tank without beating air into
the product.
EXAMPLE 1:
A direct comparison between the preservative and protectant
composition of this invention (hereinafter referred to as
"Composition A") was made with a commercial rubber and vinyl
preservative sold under the trademark ARMOR ALL and identified on
its label as falling under the claims of U.S. Pat. No. 3,956,174
(claim 3 being the only patent claim) and U.S. Pat. No. 4,133,921.
The comparative testing involved comparisons for appearance and
abrasion durability for automotive exterior vinyl trim, automobile
tires and automotive dashboards as follows:
I. AUTOMOTIVE VINYL TRIM TESTING:
Three automobiles were employed to evaluate the performance of
Composition A as compared to ARMOR ALL brand rubber preservative
and protectant. The ARMOR ALL sample was purchased at a commercial
retail establishment. The two products were compared to determine
their relative ability to provide gloss to exterior vinyl trim on
each of the three test automobiles. Prior to treatment, the
exterior vinyl trim on each car was washed with the same
commercially available detergent car wash, rinsed and dried. A
section of vinyl trim was selected at random and then taped so as
to separate the trim into two sections with a two-inch trim section
therebetween which is left untreated (control). Composition A is
applied to first section of the exterior vinyl trim and ARMOR ALL
is applied to the second section of the exterior vinyl trim. Each
vinyl trim section was treated according to the same procedure by
applying substantially the same amounts, by volume, to the area
being treated by use of a soft cloth to remove any excess
composition on the surface. After treatment the treated surfaces
were left undisturbed for 2.5 hours and then wiped with a soft
cloth. The tape was then removed from the exterior vinyl trim of
each automobile and evaluated by three judges on the basis of gloss
with each judge viewing the trim's gloss with the vinyl trim facing
the sun. The treated surfaces were evaluated for three consecutive
days to evaluate the long term affect of each composition on the
treated surface in relation to the same environmental conditions.
The third day of the evaluation included the condition of light
intermittent rain.
The judges rated the gloss of each exterior vinyl trim sample by
comparing each treated surface against the control surface and by
assigning a numerical rating to each surface as follows:
______________________________________ NUMERICAL RATING EXPLANATION
______________________________________ 2 Much better than Control 1
Better than Control 0 Equivalent to Control -1 Worse than Control
-2 Much Worse than Control
______________________________________
The resulting rating data was evaluated at a 95% confidence
interval according to the method of analyses for measurement data
as set forth in the National Bureau of Standards Handbook 91,
Chapter 3, page 3-32, published 1966, incorporated herein by
reference thereto. The results of the statistical analysis provided
values for:
n--Number of data points
.SIGMA.--Sum of Values (Measurements or ratings)
X--Average sample of n measurements
S--Standard Deviation
S.sup.2 --Square of the Standard Deviation
u--Test Criterion
As a result of this statistical analysis of the evaluation data,
Composition A was determined to provide a statistically better
gloss over the control and over ARMOR ALL under all test
conditions, including after the light rain on day three of the
test. Direct comparison of Composition A with the ARMOR ALL treated
surface (as the control) gave the following comparison for
Composition A:
______________________________________ EXTERIOR VINYL TRIM:
Frequency of Rating: .sup.(1) Rating 1st Day 2nd Day 3rd Day
______________________________________ 2 1 7 11 1 20 16 14 0 8 7 9
-1 4 4 1 -2 3 2 1 .sup.(1) Statistical Analysis: n 36 36 36
.epsilon. 12 22 33 .sup.-- X 0.3333 0.6111 0.9167 S 1.0142 1.1027
0.9673 S.sup.2 1.0286 1.2159 0.9357 Conclusion at Better than
Better than Better than 95% confidence Control Control Control
level (ARMOR (ARMOR (ARMOR ALL) ALL) ALL)
______________________________________
II. AUTOMOTIVE TIRES:
The test procedure employed for evaluation of exterior vinyl trim
was repeated using at least four judges for automotive tire
samples. Each tire was taped from top to bottom leaving a three
inch section at the top and bottom between the two tapes so as to
provide an area where the tire would not be treated with ARMOR ALL
or Composition A. In each instance, all four tires on each of four
automobiles were treated and evaluated. One of the four automobiles
was treated a second time prior to evaluation to determine the
effect of providing a second treatment of Composition A or ARMOR
ALL. The cars and tires employed were:
______________________________________ Car No. Make Year Tires
______________________________________ 1 Renault 1983 Michelin 2
Ford 1986 Michelin 3 Chevrolet 1983 Uniroyal 4* Pontiac 1989
Goodyear ______________________________________ *Automobile
receiving a second treatment
Each treated tire section was evaluated while facing the sun. The
tires were evaluated for the same three days as the exterior vinyl
trim evaluation of Part I. Direct comparison of the ARMOR ALL
treated surface (as the control) and the composition treated
surface gave the following comparison for Composition A:
______________________________________ Frequency of Rating: Rating
1st Day 2nd Day 3rd Day ______________________________________ +2 3
1 12 1 36 43 27 0 17 29 44 -1 39 23 13 -2 1 0 0 Statistical
Analysis: n 96 96 96 .epsilon. 1 22 38 .sup.-- X 0.0104 0.2292
0.3958 S 0.9787 0.8269 0.8763 S.sup.2 0.9578 1.6838 0.7680
Conclusion at Equal to Better than Better than 95% confidence
Control Control Control level (ARMOR (ARMOR (ARMOR ALL) ALL) ALL)
______________________________________
The above statistical evaluation of the test data demonstrates that
the composition according to the instant invention provided both
better initial appearance, i.e., "gloss", and better maintained
gloss after the three day test period including after exposure to
light rain.
III. INTERIOR VINYL (Dashboards):
The test procedure employed for evaluation of exterior vinyl trim
was employed to evaluate interior vinyl trim, except twelve (12)
cars were employed and each dashboard was taped to form two
sections with a two inch section between them which was not treated
(control). In addition, each tested composition was applied to six
automobiles on the driver's side of the dashboard and to the
passenger's side in the other six automobiles. The compositions
were all permitted to remain undisturbed overnight prior to wiping
the dashboard surface to remove excess composition. The automobiles
treated and the area treated were as follows:
______________________________________ COMPOSITION Auto Driver's
Passenger Automobile No. Side.sup.1 Side.sup.1
______________________________________ Black 1989 1 A ARMOR ALL
Pontiac Grand Am Dark Blue 1989 2 ARMOR ALL A Pontiac Grand Am
Maroon 1989 3 A ARMOR ALL Pontiac Grand Am Brown 1984 4 ARMOR ALL A
Chevrolet Citation Blue 1986 Ford Escort 5 A ARMOR ALL White 1983 6
A ARMOR ALL Chevrolet Citation Blue 1985 Ford Escort 7 A ARMOR ALL
Blue 1989 Oldsmobile 8 ARMOR ALL A Cutlass Salon Brown 1980 Toyota
9 ARMOR ALL A Corolla Blue 1988 Honda Acura 10 ARMOR ALL A Blue
1983 Renault 11 ARMOR ALL A Alliance White 1978 Plymouth 12 A ARMOR
ALL Volare ______________________________________ .sup.1 "A" means
the Composition A according to the instant invention.
Each treated dashboard section was evaluated and the resulting data
statistically evaluated according to the same procedure employed
for the evaluation of exterior vinyl trim in Section I of this
Example. Direct comparison of the ARMOR ALL treated surface (as the
control) to the surface treated with Composition A gave the
following comparison for Composition A:
______________________________________ Frequency of Rating: Rating
1 Day 4 Days 13 Days ______________________________________ 2 2 6
10 1 21 18 20 0 7 9 2 -1 6 3 1 -2 0 0 0 Statistical Analysis: n 36
36 33 .epsilon. 19 27 39 .sup.-- X 0.5287 0.7500 1.1818 S 0.8447
0.8409 0.6826 S.sup.2 0.7135 0.7071 0.4659 Conclusion at Better
than Better than Better than 95% confidence Control Control Control
level (ARMOR (ARMOR (ARMOR ALL) ALL) ALL)
______________________________________
The above results demonstrate that Composition A was significantly
better than ARMOR ALL in providing gloss to the interior vinyl
surfaces of the twelve automobiles.
EXAMPLE 2:
The two compositions (Composition A and ARMOR ALL) compared in
Example 2 were compared as to their relative gloss appearance
enhancement properties for sun exposed vinyl and for providing
abrasion resistance enhancement for unexposed vinyl and rubber. The
two compositions were blind as coded "Composition B" for the
commercial ARMOR ALL composition and "Composition A" for the
composition prepared according to the instant invention. The
following tests were conducted:
I. TESTS CONDUCTED: SUMMARY OF TEST RESULTS
TEST 1:
Appearance (Gloss) Measurements on exposed Vinyl testing was
conducted on exposed vinyl panels as described in Example 1.
Statistical analysis of initial gloss readings before exposure show
that at a 95% confidence level that Composition A provided better
(higher) gloss than ARMOR ALL (Composition B) and better (higher)
gloss than the untreated control. At the same time, the ARMOR ALL
treated samples were not better than the average performance of the
untreated control at a 95% confidence level.
Statistical analysis of gloss readings summarized at one, two and
three weeks, at a 95% confidence level, demonstrated that
Composition A provides a better (higher) gloss than ARMOR ALL
(Composition B).
TEST 2:
Abrasion resistance of unexposed vinyl was evaluated over a two
week period of exposure and the data summarized for one week test
intervals. At each weekly interval there was a comparison to an
untreated control, with a rating after abrasion and after
abrasion/washing. Also at each weekly interval there is a data for
direct comparisons after abrasion and after abrasion/after
washing.
Statistical analysis at a 95% confidence level for each of the test
conditions demonstrate that Composition A provided better abrasion
resistance on unexposed vinyl than ARMOR ALL (Composition B).
TEST 3:
Abrasion resistance of exposed vinyl was evaluated over a two week
period of exposure and the data summarized for one week test
intervals. At each weekly interval there was a comparison to an
untreated control, with a rating after abrasion and after
abrasion/washing. Also at each weekly interval there is a data for
direct comparisons after abrasion and after abrasion/after
washing.
Statistical analysis at a 95% confidence level for each of the test
conditions demonstrate that Composition A provided better abrasion
resistance on exposed vinyl than ARMOR ALL (Composition B).
TEST 4:
Abrasion resistance of exposed rubber was conducted over a two week
exposure period with data summarized at one week intervals. Direct
comparison for both abrasion evaluations and abrasion/washing were
made.
Statistical analysis at a 95% confidence level of the after
abrasion at one week and after two weeks show that Composition A
was better than the abrasion resistance of ARMOR ALL. Statistical
analysis at a 95% confidence level of the one week, after
abrasion/washing data show Composition A and ARMOR ALL to be
substantially equal. The statistical analysis at a 95% confidence
level of the second week, after abrasion/washing data show that
Composition A had better abrasion resistance than ARMOR ALL. These
results demonstrate the ability of Composition A to not only
provide better initial abrasion resistance than ARMOR ALL but also
to provide such protection for a longer period of time.
TEST 5:
Abrasion resistance of unexposed rubber was evaluated after
abrasion and with comparison to an untreated control and after
abrasion/washing ratings using direct sample comparisons.
Statistical analysis at a 95% confidence level demonstrated that
Composition A provided better abrasion resistance than ARMOR
ALL.
The testing procedures for Test Nos. 1, 2, 3, 4 and 5 and the
results supporting the conclusions of such tests are as
follows:
II. TEST 1: APPEARANCE TESTING
(Exposed Vinyl Panels--60 degree Gloss meter readings)
VINYL PANELS
The vinyl panels were 6".times.12" panels composed of 24 gauge cold
rolled automotive steel coated with automotive primer and covered
with GM WX4HS848 black elk grain, adhesive coated exterior
vinyl.
1. The panels are thoroughly cleaned with a commercially available
liquid car wash solution prepared following the label directions
using a sponge or cloth to wash the panels well followed by a water
rinse and drying with a soft cloth.
2. The test panel is treated with approximately 4 ml of the test
composition from a syringe to a standard applicator cloth. The
standard applicator cloth is 10".times.12" cheesecloth folded three
times to yield a pad of approximately 5".times.3". Each composition
is applied three times, evenly to the test panels using the
following sequence (except the control panels are not treated
except for the initial washing):
a. Apply the test composition, let dry 3 hours, then wipe well to
remove excess with a clean dry applicator cloth. The composition is
evenly wiped across the surface six times in the same direction
using moderate pressure sufficient to remove any excess test
composition while turning the cloth at least twice. This procedure
is repeated if an excess is still apparent upon visual inspection,
but will then be done to all samples in any set of samples, so all
samples receive the same amount of surface wiping.
b. Repeat Step a., using fresh cloth (second application).
c. Again repeat Step a., using fresh cloth (third application).
d. The test panels are then evaluated and exposed to outside
weathering.
3. a. The following scheme was used for applying the test
compositions to the numbered panels:
______________________________________ Emulsion No. Panel No.
______________________________________ Composition A 1 through 5
Composition B (ARMOR ALL) 6 through 10 Control (Untreated) 11
through 15 ______________________________________
b. The treated panels were evaluated in sets of three. Composition
A and Composition B and a control panel are assigned to each set
and shall remain in the assigned set throughout the evaluation
period:
______________________________________ Set a. Panels 1, 6 and 11
Set b. Panels 2, 7 and 12 Set c. Panels 3, 8 and 13 Set d. Panels
4, 9 and 14 Set e. Panels 5, 10 and 15
______________________________________
4. 60 degree gloss meter readings are to be taken using a Hunter
Digital Gloss Meter (Model 48-7) prior to outdoor exposure and
daily at each evaluation. The readings are recorded for each panel
including the untreated (but cleaned) control panels. Three
readings are taken on each panel.
5. Outside exposure of vinyl test panels was carried out using a GM
Black Box Test for Vinyl Top Material comprising a box (9"
(height).times.12' (length).times.8' (width)) with an open top
tilted at a five degree angle to the horizon facing south upon
which the vinyl samples are placed .
6. Panels are evaluated daily and gloss readings taken without
reapplication or cleaning until the gloss and appearance of the
treated panels were not discernibly different from that of the
untreated control panels.
7. The data was statistically analyzed as discussed in Example 1
hereof and was as follows:
______________________________________ EXPOSED VINYL PANELS 60
DEGREE GLOSS METER READINGS INITIAL READINGS BEFORE EXPOSURE
.sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 12.8 8.2 13.2 9.7 16.6 10.3
16.5 11.6 11.9 10.5 .sup.(1) Statistical Analysis: n.sub.a 5
n.sub.b 5 .epsilon..sub.a 71.00 .epsilon..sub.b 50.30 .sup.--
X.sub.a 14.20 X.sub.b 10.06 S.sub.a 2.1966 S.sub.b 1.246
S.sub.a.sup.2 4.8250 S.sub.b.sup.2 1.5530
______________________________________ BEFORE EXPOSURE EVALUATIONS
.sup.(1) COMPOSITION A UNTREATED CONTROL 12.8 9.5 13.2 9.4 16.6 9.5
16.5 9.6 11.9 9.4 .sup.(1) Statistical Analysis: n.sub.a 5 n.sub.b
5 .epsilon..sub.a 71.00 .epsilon..sub.b 47.3 .sup.-- X.sub.a 14.20
X.sub.b 9.46 S.sub.a 2.1966 S.sub.b 0.0548 S.sub.a.sup.2 4.8250
S.sub.b.sup.2 0.0030 ARMOR ALL UNTREATED CONTROL 8.2 9.5 9.7 9.4
10.3 9.5 11.6 9.6 10.5 9.4 .sup.(1) Statistical Analysis: n.sub.a 5
n.sub.b 5 .epsilon..sub.a 50.30 .epsilon..sub.b 47.3 .sup.--
X.sub.a 10.06 .sup.-- X.sub.b 9.46 S.sub.a 1.2610 S.sub.b 0.0548
S.sub.a.sup.2 1.5530 S.sub.b.sup.2 0.0030
______________________________________ FIRST SIX EVALUATIONS OVER 1
WEEK PERIOD .sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 14.3 12.0 11.9 10.8 14.5
11.3 14.3 14.7 10.7 12.3 11.3 10.0 11.4 9.8 13.8 10.5 12.3 13.5
11.0 11.5 8.2 9.4 13.9 8.0 12.9 7.6 9.8 8.8 15.1 10.7 9.9 9.6 10.6
9.7 10.0 8.5 11.2 9.7 10.3 8.4 12.7 7.1 10.0 16.0 11.4 10.4 10.6
8.5 7.8 7.3 10.2 7.8 7.6 8.4 8.7 9.6 9.8 9.2 7.8 7.9 .sup.(1)
Statistical Analysis: n.sub.a 30 n.sub.b 30 .epsilon..sub.a 334
.epsilon..sub.b 299 .sup.-- X.sub.a 11.13 .sup.-- X.sub.a 9.97
S.sub.a 2.1075 S.sub.b 2.1366 S.sub.a.sup.2 4.4416 S.sub..sup.2
4.5650 ______________________________________ 2ND SIX EVALUATION
SETS OVER 2ND WEEK PERIOD .sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 7.8 6.3 8.8 6.6 6.6 5.9 6.2
6.8 6.8 6.7 8.7 7.1 7.1 8.2 5.2 6.8 6.7 6.6 7.4 6.7 6.1 5.1 5.7 6.0
8.0 6.0 5.7 7.3 5.6 5.8 6.2 6.7 7.0 6.8 6.5 8.0 7.3 6.0 6.2 6.0 6.0
5.3 6.4 6.3 6.1 7.8 7.1 5.7 5.8 5.6 6.9 6.3 6.5 5.0 6.9 5.2 5.6 5.4
5.5 5.2 .sup.(1) Statistical Analysis: n.sub.a 30 n.sub.b 30
.epsilon..sub.a 198.4 .epsilon..sub.b 198.0 .sup.-- X.sub.a 6. 613
.sup.-- X.sub.a 6.30 S.sub.a 0.9001 S.sub.b 0.8497 S.sub.a.sup.2
0.8102 S.sub.b.sup.2 0.7221 ______________________________________
3RD EVALUATION SET 5 EVALUATIONS OVER A SIX DAY PERIOD .sup.(1)
COMPOSITION A ARMOR ALL ______________________________________ 5.0
6.5 6.6 6.0 5.8 6.5 6.5 7.1 7.0 5.5 4.9 6.0 5.0 6.0 6.4 5.4 6.6 7.5
5.3 5.5 4.8 5.1 4.8 5.8 6.2 5.0 6.5 7.3 5.0 5.3 3.8 4.3 6.0 4.7 5.6
5.0 5.5 5.3 6.4 5.3 3.5 3.8 6.7 4.6 5.4 4.8 5.4 5.1 6.3 5.4
.sup.(1) Statistical Analysis: n.sub.a 25 n.sub.b 25
.epsilon..sub.a 141.0 .epsilon..sub.b 138.8 .sup.-- X.sub.a 5.640
.sup.-- X.sub.a 5.5520 S.sub.a 0.9074 S.sub.b 0.9084 S.sub.a.sup.2
0.8233 S.sub.b.sup.2 0.8251 ______________________________________
AFTER WASHING AT END OF TEST .sup.(1) COMPOSITION A ARMOR ALL 7.0
6.1 9.8 9.4 6.6 6.1 10.3 7.8 8.5 7.9 .sup.(1) Statistical Analysis:
n.sub.a 5 n.sub.b 5 .epsilon..sub.a 42.2 .epsilon..sub.b 37.3
.sup.-- X.sub.a 8.44 .sup.-- X.sub.b 7.46 S.sub.a 1.6410 S.sub.b
1.3939 S.sub.a.sup.2 2.6930 S.sub.b.sup.2 1.9430
COMPOSITION A UNTREATED CONTROL 7.0 8.2 9.8 8.4 6.6 8.3 10.3 8.2
8.5 8.5 .sup.(1) Statistical Analysis: n.sub.a 5 n.sub.b 5
.epsilon..sub.a 42.2 .epsilon..sub.b 41.6 .sup.-- X.sub.a 8.44
.sup.-- X.sub.b 8.32 S.sub.a 1.6410 S.sub.b 0.1304 S.sub.a.sup.2
2.6930 S.sub.b.sup.2 0.0170 ARMOR ALL UNTREATED CONTROL 6.1 8.2 9.4
8.4 6.1 8.3 7.8 8.2 7.9 8.5 .sup.(1) Statistical Analysis: n.sub.a
5 n.sub.b 5 .epsilon..sub.a 37.3 .epsilon..sub.b 41.6 .sup.--
X.sub.a 7.46 .sup.-- X.sub.b 8.32 S.sub.a 1.3939 S.sub.b 0.1304
S.sub.a.sup.2 1.9430 S.sub.b.sup.2 0.0170
______________________________________
TEST 2: ABRASION TESTING
(Abrasion Resistance Test of Unexposed Vinyl
I. Materials:
1. GM specification grade WN4FB dark claret (maroon) interior vinyl
is employed as test strips (9 strips) by cutting strips from the
same large piece of vinyl with equivalent orientation.
2. No. 600 grit wet/dry sandpaper (sample supplied).
3. Gardner Straight Line Washability and Abrasion Machine, Model
No. MA-1220.
4. A commercially available liquid car wash.
II. Procedure:
1. The abrasion test employs three vinyl strips treated with
Composition A, three vinyl strips treated with Composition B and
three untreated vinyl strips as the control.
2. The vinyl strips are 4".times.18" strips cut to fit the Gardner
machine. The strips are to be first washed with a solution of a
commercially available liquid car wash, diluted according to label
directions, rinsed well with water and then dried. The vinyl strips
are then numbered in a manner whereby later identification may be
easily made.
3. Using a 5 ml syringe approximately 3 ml of the selected test
composition is evenly applied to each vinyl strip.
4. A fresh, new standard applicator cloth is used for each
application. The standard applicator cloth is a 10".times.12"
cheesecloth folded three times to yield a pad of approximately
5".times.3". Each test composition is applied three times using the
following sequence:
a. Apply the test composition to a vinyl strip, let dry for 3
hours, then wipe well to remove excess composition from the vinyl
strip. Each composition is evenly applied by wiping the applicator
across the surface six times in the same direction using moderate
pressure sufficient to remove any excess while turning the cloth at
least twice. This procedure can be repeated if test composition
excess is still visually discernable on the vinyl strip, but any
additional wiping must be done to both samples in any set, so all
vinyl samples receive the same amount of wiping.
b. Repeat Step a., using fresh cloth (second application).
c. Again repeat Step a., using fresh cloth (third application).
5. After application of Composition A or Composition B is complete,
each vinyl strip is tested as follows:
a. Pictures are taken of all vinyl strips to establish
controls.
b. A vinyl test strip is fastened to the Gardner abrasion machine
according to the machine's instructions. The No. 600 wet-dry
sandpaper is cut into 11/2".times.71/2 " strips which are wrapped
around a small piece of wood sized to fit into the aperture of the
reciprocating boat (weighing approximately 330 grams) of the
Gardner machine. The sandpaper/wood assemblage is inserted into the
boat leaving a 11/2".times.31/2" area of sandpaper to contact the
vinyl surface. A fresh, new strip of sandpaper is used to test each
vinyl strip to assure a reproducible, uniform abrasion test for
each vinyl strip without cross contamination from one test strip to
another test strip.
Each strip is abraded through fifty (or other specified number) of
cycles as measured by the Gardner machine cycle counter. The test
strips are compared to the untreated control immediately upon
completion of the abrasion test. The samples are rated according to
a rating scale.
The test strips are washed, rinsed and dried to remove any loose
debris due to the abrasion cycles. Again all the test strips are
compared to the untreated control and the ratings noted.
6. a. Rating Scale--Comparison to Untreated Control
The rating scale used is as follows:
0 Extreme abrasion--untreated control
1 Heavy abrasion
2 Medium abrasion
3 Slight abrasion--easily visible
4 Very minor abrasion
5 No abrasion
b. Direct Comparison
The two areas treated with Composition A and Composition B are
directly compared to each other with the area having the better
appearance being rated by assigning to it a 1 or 2, depending on
the degree of difference. A rating of 2 is given if there is a very
marked difference. A one rating is given when there is an easily
discernible difference. A rating of zero is given to both samples
if no discernible difference can be observed. The results of this
test were as follows:
______________________________________ ABRASION RESISTANCE OF
UNEXPOSED VINYL DIRECT COMPARISON .sup.(1) COMPOSITION A ARMOR ALL
.sup.(1,2) ______________________________________ AFTER ABRASION 2
0 1 0 2 0 .sup.(1) n.sub.a 3 n.sub.b 3 .epsilon..sub.a 5
.epsilon..sub.b 0 .sup.-- X.sub.a 1.6667 .sup.-- X.sub.b 0 S.sub.a
0.5774 S.sub.b 0 S.sub.a.sup.2 0.3333 S.sub.b.sup.2 0 AFTER WASHING
1 0 1 0 1 0 .sup.(1) Statistical Analysis: n.sub.a 3 n.sub.b 3
.epsilon..sub.a 3 .epsilon..sub.b 0 .sup.-- X.sub.a 1 .sup.--
X.sub.a 0 .sup.(2) In direct comparison testing only one product
receives a rating. Therefore, the ARMOR ALL product without the
rating is considered a zero for statistical analyses
______________________________________ values.
TEST 3: ABRASION TESTING
(Weathered-Abrasion Resistance Test of Vinyl [Exposed Vinyl])
Materials:
As in Section I of Test 2 Protocol, except that 42 test strips were
used.
Procedure:
1. Samples--same as Test 2.
2. Application-see Test 2, above, as to steps 1 to 4. This
application procedure will be used to coat 14 strips with
Composition A and 14 strips with Composition B. In addition, 14
strips remain as untreated controls samples.
3. Forty two vinyl strips are supplied to run an outdoor exposure
test, with daily evaluation. After initial application is complete
the samples are left unexposed for 24-48 hours.
4. All samples are then exposed (for 24 to 48 hours) to outdoor
weathering by attaching to open-back racks. The racks are facing
south at a 45 degree angle from horizontal.
5. A sample set consists of one each of the sample treated with
Composition A, one each of the sample treated with Composition B
and an untreated control. Each strip is then abraded (as described
in Test 2) through 25 cycles as measured by the Gardner machine
cycle counter.
Each day three vinyl strips (one set) are removed from the outdoor
racks and abrasion tested on the Gardner machine. These samples are
thereafter saved and are not returned to outdoor weathering. The
following test results were obtained:
______________________________________ ABRASION RESISTANCE OF
EXPOSED VINYL COMPARISON TO AN UNTREATED CONTROL EIGHT DATA SETS
OVER FIRST WEEK AFTER ABRASION .sup.(1,2) COMPOSITION A ARMOR ALL
______________________________________ 1 1 1 0 1 0 2 0 2 0 2 1 2 1
0 0 .sup.(1) Statistical Analysis: n.sub.a 8 n.sub.b 8
.epsilon..sub.a 5 .epsilon..sub.b 3 .sup.-- X.sub.a 1.3750 .sup.--
X.sub.b 0.3750 S.sub.a 0.7440 S.sub.b 0.5175 S.sub.a.sup.2 0.5536
S.sub.b.sup.2 0.2679 .sup.(2) The untreated control appearance is
pegged at zero and a scale of 0 to 5 is used to define relative
performance as described in the protocol for these tests.
______________________________________ SEVEN DATA SETS OVER 2ND
WEEK PERIOD AFTER ABRASION .sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 0 0 1 0 1 0 1 0 1 0 0 0 0 0
.sup.(1) Statistical Analysis: n.sub.a 7 n.sub.b 7 .epsilon..sub.a
4 .epsilon..sub.b 0 .sup.-- X.sub.a 0.5714 .sup.-- X.sub.b 0
S.sub.a 0.5345 S.sub.b 0 S.sub.a.sup.2 0.2857 S.sub.b.sup.2 0
______________________________________ EIGHT DATA SETS OVER FIRST
WEEK AFTER ABRASION AND AFTER WASHING .sup.(1) COMPOSITION A ARMOR
ALL ______________________________________ 3 2 2 0 1 0 2 0 2 0 2 0
2 0 1 0 .sup.(1) Statistical Analysis: n.sub.a 8 n.sub.b 8
.epsilon..sub.a 15 .epsilon..sub.b 2 .sup.-- X.sub.a 0.8750 .sup.--
X.sub. b 0.2500 S.sub.a 0.6409 S.sub.b 0.7071 S.sub.a.sup.2 0.4107
S.sub.b.sup.2 0.5000 ______________________________________ SEVEN
DATA SETS OVER 2ND WEEK PERIOD AFTER ABRASION AND AFTER WASHING
.sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 1 0 1 0 2 0 1 0 2 1 2 0 2 0
1 0 .sup.(1) Statistical Analysis: n.sub.a 7 n.sub.b 7
.epsilon..sub.a 11 .epsilon..sub.b 1 .sup.-- X.sub.a 1.5714 .sup.--
X.sub.b 0.1429 S.sub.a 0.5345 S.sub.b 0.3780 S.sub.a.sup.2 0.2857
S.sub.b.sup.2 0.1429 ______________________________________
ABRASION RESISTANCE OF EXPOSED VINYL DIRECT COMPARISON RATING
.sup.(1,2) EIGHT DATA SETS OVER FIRST WEEK AFTER ABRASION
COMPOSITION A ARMOR ALL ______________________________________ 1 0
2 0 2 0 2 0 2 0 1 0 2 0 1 0 .sup.(1) Statistical Analysis: n.sub.a
8 n.sub.b 8 .epsilon..sub.a 13 .epsilon..sub.b 0 .sup.-- X.sub.a
1.6250 .sup.-- X.sub.b 0 S.sub.a 0.5175 S.sub.b 0 S.sub.a.sup.2
0.2678 S.sub.b.sup.2 0 .sup.(2) Direct comparison rating-only one
product receives a value of 1 or 2 and the other is zero. If both
are equal, they are both rated zero. Rating scale details are
described in the protocol for these tests.
______________________________________ SEVEN DATA SETS OVER 2ND
WEEK PERIOD AFTER ABRASION .sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 2 0 1 0 1 0 1 0 1 0 1 0 1 0
1 0 .sup.(1) Statistical Analysis: n.sub.a 7 n.sub. b 7
.epsilon..sub.a 8 .epsilon..sub.b 0 .sup.-- X.sub.a 1.1429 .sup.--
X.sub.b 0 S.sub.a 0.3780 S.sub.b 0 S.sub.a.sup.2 0.1429
S.sub.b.sup.2 0 ______________________________________ EIGHT DATA
SETS OVER FIRST WEEK PERIOD AFTER ABRASION AND AFTER WASHING
.sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 1 0 2 0 2 0 2 0 1 0 0 0 2 0
1 0 .sup.(1) Statistical Analysis: n.sub.a 8 n.sub.b 8
.epsilon..sub.a 11 .epsilon..sub.b 0 .sup.-- X.sub.a 1.3750 .sup.--
X.sub.b 0 S.sub.a 0.7440 S.sub.b 0 S.sub.a.sup.2 0.5536
S.sub.b.sup.2 0 ______________________________________ SEVEN DATA
SETS OVER 2ND WEEK PERIOD AFTER ABRASION AND AFTER WASHING .sup.(1)
COMPOSITION A ARMOR ALL ______________________________________ 2 0
0 0 0 0 1 0 1 0 1 0 1 0 .sup.(1) Statistical Analysis: n.sub.a 7
n.sub.b 7 .epsilon..sub.a 6 .epsilon..sub.b 0 .sup.-- X.sub.a
1.8571 .sup.-- X.sub.b 0 S.sub.a 0.6901 S.sub.b 0 S.sub.a.sup.2
0.4762 S.sub.b.sup.2 0 ______________________________________
TEST 4: ABRASION TESTING
(Weathered-Abrasion Resistance Test of Rubber (Exposed Rubber))
Materials:
Forty two (42) synthetic rubber strips.
Procedure:
1. Samples--prepared as in Test 3.
2. Application--Test 2 procedure employed. This application
procedure is used to treat 14 strips with Composition A and 14
strips with Composition B. In addition 14 strips remain as
untreated controls.
3. Forty two rubber strips are supplied to run an exposure test,
with daily evaluation.
4. After application, all samples were exposed to outdoor
weathering by attaching to open-back racks. The racks are facing
south at a 45 degree angle from horizontal.
5. A sample set consists of one each of the sample treated with
Composition A, one each sample treated with Composition B and an
untreated control. Each strip is abraded through cycles as measured
by the Gardner machine cycle counter (the procedure as per Test
2).
Each day three rubber strips (one set) are removed from the outdoor
racks and abrasion tested on the Gardner machine. These are
thereafter saved and not returned to outdoor weathering.
______________________________________ ABRASION RESISTANCE OF
EXPOSED RUBBER DIRECT COMPARISON RATING .sup.(1,2) SEVEN DATA SETS
FIRST WEEK AFTER ABRASION COMPOSITION A ARMOR ALL
______________________________________ 1 0 2 0 2 0 2 0 2 0 2 0 2 0
.sup.(1) Statistical Analysis: n.sub.a 7 n.sub.b 7 .epsilon..sub.a
13 .epsilon..sub.b 0 .sup.-- X.sub.a 1.8571 .sup.-- X.sub.b 0
S.sub.a 0.3780 S.sub.b 0 S.sub.a.sup.2 0.1429 S.sub.b.sup.2 0
.sup.(2) Direct comparison rating-only one product receives a value
of 1 or 2 and the other is zero. If both are equal, they are both
rated zero. Rating scale details are described in the protocol for
these tests. ______________________________________ ABRASION
RESISTANCE OF EXPOSED RUBBER DIRECT COMPARISON RATINGS SEVEN DATA
SETS 2ND WEEK AFTER ABRASION .sup.(1) COMPOSITION A ARMOR ALL
______________________________________ 2 0 2 0 2 0 2 0 2 0 2 0 2 0
.sup.(1) Statistical Analysis: n.sub.a 7 n.sub.b 7 .epsilon..sub.a
14 .epsilon..sub.b 0 .sup.-- X.sub.a 2 .sup.-- X.sub.b 0
______________________________________ SEVEN DATA SETS OF THREE,
FIRST WFEK AFTER ABRASION AND AFTER WASHING .sup.(1,2) COMPOSITION
A ARMOR ALL ______________________________________ 1 0 0 1 0 0 0 0
0 0 0 0 0 0 0 0 1 0 0 0 0 1 0 0 1 0 0 0 0 0 0 0 1 0 .sup.(1)
Statistical Analysis: n.sub.a 21 n.sub. b 21 .epsilon..sub.a 8
.epsilon..sub.b 6 .sup.-- X.sub.a 0.3810 .sup.-- X.sub.b 0.2857
S.sub.a 0.4976 S.sub.b 0.4629 S.sub.a.sup.2 0.2476 S.sub.b.sup.2
0.2143 .sup.(2) Evaluations made by three independent observers per
______________________________________ day. SEVEN DATA SETS OF
THREE, 2ND WEEK AFTER ABRASION AND AFTER WASHING .sup.(1)
COMPOSITION A ARMOR ALL ______________________________________ 0 0
1 0 1 0 1 0 1 0 0 1 1 0 1 0 1 0 2 0 1 0 0 0 1 0 1 0 0 0 2 0 1 0 0 0
1 0 1 0 .sup.(1) Statistical Analysis: n.sub.a 21 n.sub.b 21
.epsilon..sub.a 17 .epsilon..sub. b 2 .sup.-- X.sub.a 0.8095
.sup.-- X.sub.b 0.0952 S.sub.a 0.6016 S.sub.b 0.3008 S.sub.a.sup.2
0.3619 S.sub.b.sup.2 0.0905
______________________________________
TEST 5: ABRASION TESTING
(Abrasion Resistance Test of Unexposed Rubber Strips)
I. Materials:
1. Hi-Grade black neoprene rubber meeting ASTM-D-2000-75 Type BC
having a hardness of shore A durometer-35-45A soft, 1/8" thick.
2. No. 600 grit wet/dry sandpaper.
3. Gardner Straight Line Washability and Abrasion Machine, Model
No. MA-1220.
4. Commonly available commercial liquid car wash.
II. Procedure:
1. The test consists of three rubber strips treated with
Composition A, three treated with Composition B and three untreated
controls.
2. The rubber strips are 4".times.18" strips to fit the Gardner
machine. The strips are first washed with a solution of
commercially available liquid car wash diluted according to label
directions, rinsed well with water and then dried. The rubber
strips are then numbered in a manner whereby later identification
can be easily made.
3. Using a 5 ml syringe, approximately 3 ml of a test composition
is applied to each rubber strip sample.
4. A fresh, new standard applicator cloth is used for each
application. The standard applicator cloth is a 10".times.12"
cheesecloth folded three times to yield a pad of approximately
5".times.3". Each test composition is applied three times to a
rubber test strip using the following sequence:
a. Apply the test composition, let it dry for a selected period of
3 to 24 hours, then wipe well to remove excess with a clean dry
cloth. The wipe procedure uses a single fresh applicator cloth. The
sample is evenly wiped across the surface six times in the same
direction using moderate pressure sufficient to remove any excess,
turning the cloth at least twice. This procedure can be repeated if
an excess is still visually observable, but must be repeated for
all treated samples in any set, so that all samples receive the
same amount of surface wiping.
b. Repeat Step a., using a fresh cloth (second application).
c. Again repeat Step a., using a fresh cloth (third
application).
5. After application is complete, abrasion testing is conducted as
described above in Test 2.
6. The data is then statistically analyzed. The following results
were obtained:
______________________________________ COMPOSITION A ARMOR ALL
______________________________________ ABRASION RESISTANCE OF
UNEXPOSED RUBBER COMPARED TO AN UNTREATED CONTROL AFTER ABRASION
.sup.(1) 2 1 2 1 2 1 .sup.(1) Statistical Analysis: n.sub.a 3
n.sub.b 3 .epsilon..sub.a 6 .epsilon..sub.b 3 .sup.-- X.sub.a 2
.sup.-- X.sub.b 1 ABRASION RESISTANCE OF UNEXPOSED RUBBER DIRECT
COMPARISON AFTER ABRASION .sup.(1) 1 0 1 0 1 0 .sup.(1) Statistical
Analysis: n.sub.a 3 n.sub.b 3 .epsilon..sub.a 3 .epsilon..sub.b 0
.sup.-- X.sub.a 1 .sup.-- X.sub.b 0
______________________________________
__________________________________________________________________________
EXAMPLE 3: DATA SUMMARY STAT. ANAL. TEST TREATED TEST TEST AT 95%
CONF. NO. SUBSTRATE TEST EVALUATION TYPE.sup.(1) DATA LEVEL
__________________________________________________________________________
1 Black ext. Exposed Daily/3 weeks Appearance 60.degree. Gloss
Composition A Vinyl GM Black Meter Read. Better than Box Test ARMOR
ALL 2 Maroon ext. Unexposed 3 Hrs after last Abrasion Comparison to
Composition A Vinyl Application Resistance Untreated Better than
Control & ARMOR ALL Direct Compar. Ratings 3 Maroon int.
Exposed Daily/2 weeks Abrasion Comparison to Composition A Vinyl
Resistance Untreated Better than Control & ARMOR ALL Direct
Compar. Ratings 4 Rubber Exposed Daily/2 weeks Abrasion Direct
Composition A Resistance Comparison Better than Ratings ARMOR ALL 5
Rubber Unexposed 3 Hrs. after last Abrasion Comparison to
Composition A Application Resistance Untreated Better than Control
& ARMOR ALL Direct Compar. Ratings
__________________________________________________________________________
.sup.(1) Test Type = Appearance measured by Gloss Meter readings
which show whether product had a higher gloss, i.e., better
appearance. Abrasion Resistance = Gardner testing showed if product
gave better resistance to abrasion.
EXAMPLE 3:
(a) The test procedure for evaluating surface abrasion of treated
vinyl panels (General Motor's specification grade maroon interior
vinyl) was carried out according to the procedure of Example 2,
Test 2, using the following compositions:
______________________________________ Test Composition No.
Composition ______________________________________ 1 ARMOR ALL 2
TURTLE CLEAR GUARD 3 COMPOSITION A 4 NU VINYL 5 COMPOSITION C* 6
RAINDANCE PROTECTANT ______________________________________
*Composition C is a commercially available protestant containing:
about 75 wt % water about 20 wt % dimethylpolysiloxane (provided as
an emulsion [60 wt. % dimethylpolysiloxane]) about 5 wt % propylene
glycol
After abrasion testing using a Gardner Straight Line Washability
and Abrasion Machine, the following relative ratings were
obtained:
______________________________________ Product Product Product
Tested Rating.sup.1,2 Rating.sup.1,3
______________________________________ ARMOR ALL 3 3 TURTLE CLEAR
GUARD 2 1 COMPOSITION A 5 5 NU VINYL 2 2 COMPOSITION C 3 3
RAINDANCE PROTECTANT 3 3 CONTROL (UNTREATED) 0 0
______________________________________ .sup.1 Ratings are: 0 =
Extreme Abrasion (Untreated Control) 1 = Heavy Abrasion 2 = Medium
Abrasion 3 = Slight Abrasion 4 = Minor Abrasion 5 = No Abrasion
.sup.2 Ratings after excess being wiped after 2.5 hours. .sup.3
Ratings after excess being wiped after setting overnight.
The above procedure was again followed except the treated vinyl
strips were given two applications of the selected compositions by
wiping excess composition from each vinyl strip after 2.5 hours and
then applying a treatment with the composition and permitting such
to set overnight before the excess composition from the second
application is wiped from treated surface. The abrasion testing for
each strip having two treatments is then conducted as discussed
above. Each of the above compositions received the following
ratings (as defined above):
______________________________________ Product Rating
______________________________________ ARMOR ALL 2 TURTLE CLEAR
GUARD 1 COMPOSITION A 5 COMPOSITION C 3 RAINDANCE PROTECTANT 2
CONTROL (UNTREATED) 0 ______________________________________
(b) The general test procedure of part (a) for abrasion testing was
employed to evaluate the retained gloss of General Motor's
specification grade maroon interior vinyl after a specified number
of washing cycles using a Gardner Straight Line Washability and
Abrasion Machine. In this test, cellulose sponge for washing is
substituted for the sandpaper and a commercially available car wash
concentrate is diluted on the basis of one ounce per gallon of
water. The cellulose sponge is 3.25 inch .times.1.125 inch
.times.1.25 inch and weighed about 8.92 grams. The cellulose sponge
was affixed to the 330 gram boat in place of the sandpaper
described in the abrasion resistance testing. Fifteen (15)
mililiters of the diluted commercial car wash was applied to the
sponge before the selected number of washing cycles is commenced.
After the washing cycles are completed the panel is rinsed with
water and evaluated. A total of sixteen (16) panels were evaluated
for three different compositions with the evaluation of a panel
being reported as either "GR" for "Gloss Retained" or "GL" for
Gloss Lost". The results were as follows:
______________________________________ Washing Composition Tested
Cycles ARMOR ALL Composition A Composition C
______________________________________ 5 GL GR.sup.1 GL 10 GL.sup.1
GR.sup.2 GL.sup.1 25 GL GR.sup.1 GL
______________________________________ .sup.1 Average of two tests.
.sup.2 Average of four tests.
* * * * *